CN113956899B - Method for removing impurities from coal tar - Google Patents
Method for removing impurities from coal tar Download PDFInfo
- Publication number
- CN113956899B CN113956899B CN202111394481.5A CN202111394481A CN113956899B CN 113956899 B CN113956899 B CN 113956899B CN 202111394481 A CN202111394481 A CN 202111394481A CN 113956899 B CN113956899 B CN 113956899B
- Authority
- CN
- China
- Prior art keywords
- coal tar
- stirring
- water
- temperature
- shell
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
- C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/022—Metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Manufacturing & Machinery (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention belongs to the technical field of coal chemical industry, and discloses a method for removing impurities from coal tar, which comprises the following steps: s1, filtering coal tar through a filter membrane to obtain filtered coal tar, and uniformly stirring the filtered coal tar and a demetallizing agent through a stirring device to convert a metal complex and organic chlorine in the filtered coal tar into inorganic salt; then adding water into the coal tar, and uniformly stirring the mixture by a stirring device to ensure that the converted inorganic salt is transferred from the coal tar to a water phase to obtain a mixture; s2, separating the mixture into three phases of solid, water and oil by a horizontal screw centrifuge, and then removing residual water from the oil phase by centrifugal flash evaporation to obtain the coal tar without impurities. The method can improve the quality of the coal tar, reduce the running cost of the downstream hydrogenation device and prolong the running period of the downstream hydrogenation device.
Description
Technical Field
The invention relates to the technical field of coal chemical industry, in particular to a method for removing impurities from coal tar.
Background
The coal tar is a product obtained by dry distillation when coke is produced by coal in a coking plant, and a large amount of water, metal, salt and chlorine are carried in the coal tar. The carrying of water can cause the pumping out of a feeding pump of a downstream hydrogenation device and the damage to the mechanical property of a catalyst; the carrying of metal causes the surface adsorption or pore channel blockage of the downstream hydrogenation device catalyst, and the activity is rapidly reduced; the salt (calculated by sodium chloride) and chlorine react with hydrogen and ammonia to generate ammonium chloride, so that the ammonium chloride is separated out and crystallized, and the chlorine corrodes related equipment and pipelines after reaching the dew point, so that the impurities greatly reduce the long-period stable operation of downstream devices, reduce the service life of hydrogenation catalysts and increase the operation cost.
At present, the domestic coal tar impurity removal is mainly carried out step by step, and demetallization is realized by adding a demetallization agent and then carrying out filter pressing and centrifugal deslagging; dehydration in coal tar is realized through atmospheric and vacuum distillation and coalescence; the desalting treatment in the coal tar is realized by water washing after electrolysis, however, in actual operation, the treatment methods have the problems of large sewage quantity, high difficulty in oil-water emulsification separation, unstable operation and the like, and therefore, the invention provides the method for removing impurities from the coal tar.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a method for removing impurities from coal tar.
The method for removing impurities from coal tar is realized by the following technical scheme:
a method for removing impurities from coal tar comprises the following steps:
s1, filtering coal tar through a filter membrane, removing heavy asphaltene in medium-low temperature coal tar, and removing to obtain filtered coal tar; then uniformly stirring the filtered coal tar and the demetallization agent by a stirring device, so that a metal complex and organic chlorine in the filtered coal tar are converted into inorganic salt to obtain a first mixture; adding water into the first mixture, and uniformly stirring by using a stirring device to transfer the converted inorganic salt from the coal tar into a water phase to obtain a second mixture;
s2, separating the second mixture into solid residue, water and oil phases by a horizontal screw centrifuge to obtain a solid phase, a water phase and an oil phase; and then filtering residual solid impurities from the oil phase by a multistage filter, and removing residual moisture from the oil phase by centrifugal flash evaporation treatment to obtain the coal tar without impurities.
Further, the stirring device includes:
the upper end of the shell is provided with an oil inlet, a chemical inlet, a water inlet mechanism and a driving mechanism; a stirring mechanism is arranged in the stirring device; and the lower end of the discharge hole is provided with a discharge hole;
the stirring mechanism comprises a rotating rod, a plurality of stirring rods and a plurality of wall scrapers;
the rotating rod is vertically arranged in the shell, and the upper end of the rotating rod penetrates through the shell to be in transmission connection with the driving mechanism;
the stirring rods are arranged at equal intervals along the axial direction of the rotating rod, one end of each stirring rod is fixedly connected with the rotating rod, and the other end of each two adjacent stirring rods in the vertical direction is fixedly connected with one side of one wall scraper; the other side of the wall scraper is abutted against the side wall of the shell.
Further, the driving mechanism comprises a mounting block, a first gear, a second gear, a linkage rod and a driving motor; the mounting block is arranged in a mounting groove formed in the upper end of the shell, the lower end of the mounting block is fixedly connected with the rotating rod, the upper end of the mounting block is fixedly connected with the first gear, and the second gear is in meshed connection with the first gear; one end of the linkage rod is fixedly arranged on a rotating axis of the second gear, the other end of the linkage rod is connected with the driving motor, and the driving motor is used for driving the linkage rod to rotate.
Further, the water inlet mechanism includes:
one end of the water inlet pipe is used for connecting a water source, and the other end of the water inlet pipe is provided with a three-way valve;
the two flow guide pipes are respectively arranged at two symmetrical water outlet ends of the three-way valve;
the two spray heads are respectively arranged at the water outlet ends of the two flow guide pipes;
and the two first valve bodies are respectively arranged on the two flow guide pipes and respectively positioned between the three-way valve and the two spray heads.
Further, the device also comprises a heating mechanism and a heat dissipation mechanism;
the heating mechanism comprises an electric heating piece and a temperature sensor, and the electric heating piece is sleeved on the inner wall of the shell; the temperature sensor is arranged at the bottom of the inner side of the shell;
the heat dissipation mechanism comprises a ventilation cavity, the ventilation cavity is arranged between the electric heating piece and the outer wall of the shell, an air inlet is formed in one end of the ventilation cavity, and an air outlet is formed in the other end of the ventilation cavity; the air inlet and the air outlet are respectively provided with a second valve body and a third valve body
Furthermore, the lower end of the rotating rod is also horizontally provided with an auxiliary stirring rod.
Furthermore, the oil inlet, the agent inlet and the discharge port are all provided with a first control valve body.
Further, the filtering membrane is prepared by the following steps:
step 1, weighing the following preparation raw materials in parts by weight for later use: 45 to 50 parts of Al metal powder, 35 to 40 parts of Nb metal powder, 5 to 10 parts of Ti metal powder and Y 2 O 3 5-10 parts of nano particles;
and 3, under a vacuum condition, heating the pressed blank from room temperature to 120 ℃ at a heating rate of 3-5 ℃/min, preserving heat for 0.5-1.5 h, then heating to 550-650 ℃ at a heating rate of 2-4 ℃/min, preserving heat for 3-5 h, then heating to 850-950 ℃ at a heating rate of 2-4 ℃/min, preserving heat for 3-5 h, heating to 1250-1350 ℃ at a heating rate of 3-5 ℃/min, preserving heat for 3-5 h, and cooling to obtain the filtering membrane.
Further, the demetallizing agent is a polyamine carboxylate.
Furthermore, the dosage ratio of the demetallization agent to the coal tar is 100-200 mug: 1g.
Further, the stirring temperature after the demetallization agent is added into the S2 is 60-80 ℃; the stirring temperature after the metal removing agent is added is 75-85 ℃.
Further, heating the medium-low temperature coal tar to 50-65 ℃, and then filtering with a filter membrane.
Further, the demetallizing agent is one or two of nitrilotriacetic acid and ethylene diamine tetraacetic acid disodium.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the coal tar is filtered by the filter membrane to remove heavy asphaltenes in the coal tar, so that the two-phase interface liquid membrane of water drops stably coated by oil and stabilized by the solid particles is destroyed while the content of the heavy asphaltenes in the coal tar is reduced, the demulsification effect of the coal tar is realized, and the subsequent separation treatment is facilitated.
The coal tar after filtration and the demetallizing agent are placed in a stirring device together, the demetallizing agent and the coal tar after filtration are in full contact reaction through the stirring device, and a metal complex and organic chlorine in the coal tar after filtration are converted into inorganic salt capable of being dissolved in water, so that a first mixture is obtained. And then adding water into the first mixture, and stirring and mixing the mixture fully by a stirring device to dissolve the converted inorganic salt in the water, so that the metal and chlorine in the coal tar are transferred into a water phase to obtain a second mixture.
And then the second mixture is subjected to high-speed centrifugation by controlling the rotating speed of a horizontal screw centrifuge, so that solid-phase substances with higher density are separated by an outermost rotary drum, water with lower density is discharged from a sewage port at the innermost side, coal tar is separated from the middle, three-phase separation of solid, water and oil is realized, the separated coal tar is dehydrated by centrifugal flash evaporation, and the dehydration in the coal tar is further realized.
According to the invention, the metal powders are uniformly mixed and then sintered, and the Al, nb and Ti metal powders are enabled to form the micron-sized three-dimensional porous support body and Y is enabled to be simultaneously used for carrying out Y-shaped porous support body through the mutual diffusion and restriction of multiple elements and the synergistic and sequential sectional sintering 2 O 3 The nano particles gradually react with the micron-sized three-dimensional porous support body, and a nano-scale three-dimensional reticular structure is constructed on the micron-sized three-dimensional porous support body, so that the micron/nano dual-scale filtering membrane is formed. In addition, the invention can restrict the diffusion of various intermediate products formed after the diffusion of each element by controlling the heating rate and the heat preservation time of each sintering stage, thereby realizing the control of the aperture size of the filtering membrane and further ensuring the removal of heavy asphaltene in the coal tar.
The method can improve the quality of coal tar, reduce the operation cost of the downstream hydrogenation device and prolong the operation period of the downstream hydrogenation device.
Drawings
FIG. 1 is a schematic structural view of a stirring apparatus of the present invention.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
Example 1
The embodiment provides a method for removing impurities from coal tar, which comprises the following steps:
s1, heating the coal tar to 60 ℃ through a heat exchanger, and then filtering the coal tar through a filter membrane to remove heavy asphaltene in the coal tar, so that the heavy asphaltene content in the coal tar is reduced, and meanwhile, a two-phase interface liquid membrane of water drops stably coated by oil and stabilized by solid particles is destroyed, the demulsification effect of the coal tar is realized, and the subsequent separation treatment is facilitated.
And then, putting the filtered coal tar and the demetallization agent into a stirring device, stirring for 2 hours at the temperature of 70 ℃ and at the rotating speed of 300r/min, so that the demetallization agent and the filtered coal tar are in full contact reaction, and converting a metal complex and organic chlorine in the filtered coal tar into inorganic salt capable of being dissolved in water to obtain a first mixture. And then adding water into the first mixture, adjusting the temperature of a stirring device to 80 ℃, and stirring at a rotating speed of 300r/min for 2.5 hours to dissolve the converted inorganic salt in the water, so that the metal and chlorine in the coal tar are transferred to a water phase to obtain a second mixture.
And controlling the rotating speed of a horizontal decanter centrifuge to 3000r/min to separate a solid phase substance with higher density from an outermost rotating drum, discharging water with lower density from a sewage port at the innermost side, separating coal tar from the middle to realize three-phase separation of solid, water and oil, heating the separated coal tar to 130 ℃ through a heat exchanger, and then performing centrifugal flash evaporation dehydration to further realize dehydration in the coal tar.
In the embodiment, the dosage ratio of the demetallizing agent to the coal tar is 150 mug to 1g.
In this embodiment, the demetallizing agent is nitrilotriacetic acid.
Example 2
The embodiment provides a method for removing impurities from coal tar, which comprises the following steps:
s1, heating coal tar to 50 ℃ through a heat exchanger, and filtering the coal tar with a filter membrane to remove heavy asphaltenes in the coal tar, so that the two-phase interface liquid membrane of water drops stably bound by oil and contained by solid particles is destroyed while the content of the heavy asphaltenes in the coal tar is reduced, the demulsification effect of the coal tar is realized, and the subsequent separation treatment is facilitated.
Then, the filtered coal tar and the demetallization agent are placed in a stirring device together, and the mixture is stirred for 3 hours at the temperature of 60 ℃ and at the rotating speed of 250r/min, so that the demetallization agent and the filtered coal tar are in full contact reaction, and a metal complex and organic chlorine in the filtered coal tar are converted into inorganic salt capable of being dissolved in water, and a first mixture is obtained. And then adding water into the first mixture, adjusting the temperature of a stirring device to 75 ℃, and stirring at a rotating speed of 250r/min for 3h to dissolve the converted inorganic salt in the water, so that the metal and chlorine in the coal tar are transferred to a water phase to obtain a second mixture.
And then the second mixture is subjected to rotation speed control of a horizontal screw centrifuge at 2800r/min, so that solid phase substances with high density are separated through an outermost rotary drum, water with low density is discharged through a sewage port at the innermost side, coal tar is separated out from the middle, three-phase separation of solid, water and oil is realized, the separated coal tar is heated to 120 ℃ through a heat exchanger and then subjected to centrifugal flash evaporation dehydration, and further dehydration in the coal tar is realized.
In this example, the ratio of the amount of the demetallizing agent to the amount of the coal tar was 100. Mu.g: 1g.
In this embodiment, the demetallizing agent is nitrilotriacetic acid.
Example 3
The embodiment provides a method for removing impurities from coal tar, which comprises the following steps:
s1, heating the coal tar to 65 ℃ through a heat exchanger, and then filtering the coal tar through a filter membrane to remove heavy asphaltene in the coal tar, so that the heavy asphaltene content in the coal tar is reduced, and meanwhile, a two-phase interface liquid membrane of water drops stably coated by oil and stabilized by solid particles is destroyed, the demulsification effect of the coal tar is realized, and the subsequent separation treatment is facilitated.
Then, the filtered coal tar and the demetallization agent are placed in a stirring device together, and the mixture is stirred for 0.5 hour at the temperature of 80 ℃ and at the rotating speed of 300r/min, so that the demetallization agent and the filtered coal tar are in full contact reaction, and a metal complex and organic chlorine in the filtered coal tar are converted into inorganic salt capable of being dissolved in water, and a first mixture is obtained. And then adding water into the first mixture, and stirring for 0.5h at the rotating speed of 300r/min by adjusting the temperature of a stirring device to 85 ℃ so as to dissolve the converted inorganic salt in the water, thereby transferring the metal and chlorine in the coal tar into the water phase to obtain a second mixture.
And then, controlling the rotating speed of a horizontal screw centrifuge to 3300r/min, so that the solid phase substance with higher density is separated by an outermost rotary drum, the water with lower density is discharged through a sewage port at the innermost side, the coal tar is separated from the middle, solid, water and oil three-phase separation is realized, the separated coal tar is heated to 140 ℃ by a heat exchanger, and then is subjected to centrifugal flash evaporation dehydration, and further dehydration in the coal tar is realized.
In this example, the ratio of the amount of the demetallizing agent to the amount of the coal tar was 200. Mu.g: 1g.
In this embodiment, the demetallizing agent is disodium edetate.
Example 4
The stirring processes of embodiments 1 to 3 are all realized by the stirring apparatus of this embodiment, referring to fig. 1, the stirring apparatus of this embodiment includes:
an oil inlet 11, a chemical inlet 11, a water inlet mechanism 2 and a driving mechanism 3 are arranged at the upper end of the shell 1; the inside of the stirring mechanism is provided with a stirring mechanism 4; and the lower end is provided with a discharge hole 13;
the stirring mechanism 4 includes a rotating lever 41, a plurality of stirring levers 42, and a plurality of wall scrapers 43; the rotating rod 41 is vertically arranged in the housing 1; a plurality of stirring rods 42 are arranged at equal intervals along the axial direction of the rotating rod 41, one end of each stirring rod 42 is fixedly connected with the rotating rod 41, and the other end of each two adjacent stirring rods 42 in the vertical direction is fixedly connected with one side of one wall scraper 43; the other side of the wall scraper 43 abuts against the side wall of the housing 1;
the driving mechanism 3 comprises a mounting block 31, a first gear 32, a second gear 33, a linkage 34 and a driving motor 35; the mounting block 31 is arranged in the mounting groove 14 formed at the upper end of the shell 1, the lower end of the mounting block is fixedly connected with the rotating rod 41, the upper end of the mounting block is fixedly connected with the first gear 32, and the second gear 33 is meshed with the first gear 32; one end of the linkage 34 is fixedly arranged on the rotation axis of the second gear 33, the other end of the linkage 34 is connected with the driving motor 35, and the driving motor 35 is used for driving the linkage 34 to rotate.
In the stirring process, the discharge port 13 is in a closed state, the coal tar subjected to filtering treatment is added into the stirring device of the embodiment through the oil inlet 11, then the demetallizing agent is added through the agent inlet 11, the driving motor is started to drive the linkage rod 34 to rotate, the linkage rod 34 rotates to drive the second gear 33 to rotate, the second gear 33 rotates to drive the first gear 32 to rotate, the first gear 32 rotates to drive the installation block 31 to rotate, the installation block 31 rotates to drive the rotating rod 41 to rotate, further, the stirring rod 42 is driven to rotate to stir and mix the materials inside the shell 1, meanwhile, the wall scraper 43 rotates along with the rotating rod 41, thereby scraping and sweeping the materials on the inner wall of the shell 1, adhesion of the materials on the inner wall of the shell 1 is avoided, and uniform stirring of the materials is realized while material loss is avoided.
In order to avoid uneven stirring of the materials at the bottom of the casing 1, the present embodiment is further horizontally provided with an auxiliary stirring rod 44 at the lower end of the rotating rod 41.
In order to ensure that the water removes the salt in the mixed material, the water inlet mechanism 2 of a preferred embodiment of the invention comprises:
a water inlet pipe 21, one end of which is used for connecting a water source and the other end of which is provided with a three-way valve 22;
the two flow guide pipes 23 are respectively arranged at two symmetrical water outlet ends of the three-way valve 22;
the two spray heads 24 are respectively arranged at the water outlet ends of the two flow guide pipes 23;
the two first valve bodies 25 are respectively disposed on the two flow guide pipes 23 and respectively located between the three-way valve 22 and the two nozzles 24.
The inner wall of the shell 1 is washed by the spray head 24, so that water is fully contacted with inorganic salt in the mixed material, and the mixed material is fully reacted under the stirring of the stirring mechanism 4, and further, the removal of metal and organic chlorine in the coal tar is ensured. The water adding and the water adding stopping can be realized by controlling the switches of the two first valve bodies 25.
In order to facilitate the regulation of the temperature of the stirring device according to the requirement, the stirring device of a preferred embodiment of the present invention further comprises a heating mechanism 5 and a heat dissipation mechanism 6.
The heating mechanism 5 of the present embodiment includes an electric heating sheet 51 and a temperature sensor 52, wherein the electric heating sheet 51 of the present embodiment is sleeved on the inner wall of the casing 1; the temperature sensor 52 is provided at the bottom inside the casing 1. The shell 1 is heated through the electric heating sheet 51, and meanwhile, the temperature sensor 52 monitors the temperature inside the shell 1, so that the temperature of the shell 1 is controlled, and the situation that the removal effect is influenced due to overhigh or overlow stirring temperature is avoided.
The heat dissipation mechanism 6 of the present embodiment includes a ventilation chamber 61, the ventilation chamber 61 is disposed between the electric heating element 51 and the outer wall of the housing 1, an air inlet 62 is disposed at one end of the ventilation chamber 61, an air outlet 63 is disposed at the other end of the ventilation chamber 61, and a second valve body 64 and a third valve body 65 are disposed on the air inlet 62 and the air outlet 63, respectively. Through opening second valve body 64 and third valve body 65 simultaneously for ventilation chamber 61 and external intercommunication, can realize the circulation of air in the ventilation chamber 61, dispel the heat through the air of circulation to casing 1, thereby avoid stirring the condition appearance of high temperature. And for quick heat dissipation, the air inlet 62 can be communicated with cold air, so as to realize quick cooling.
It should be noted that the filtration membrane in each of the above examples is prepared by the following steps:
step 1, according to the following weightWeighing the preparation raw materials in parts by weight for later use: 45 to 50 parts of Al metal powder, 35 to 40 parts of Nb metal powder, 5 to 10 parts of Ti metal powder and Y 2 O 3 5-10 parts of nano particles;
and 3, under the vacuum condition, heating the pressed compact from room temperature to 120 ℃ at the heating rate of 3-5 ℃/min and preserving heat for 0.5-1.5 h, then heating to 550-650 ℃ at the heating rate of 2-4 ℃/min and preserving heat for 3-5 h, then heating to 850-950 ℃ at the heating rate of 2-4 ℃/min and preserving heat for 3-5 h, heating to 1250-1350 ℃ at the heating rate of 3-5 ℃/min and preserving heat for 3-5 h, and cooling to obtain the filtering membrane.
According to the invention, the metal powders are uniformly mixed and then sintered, and the Al, nb and Ti metal powders are enabled to form the micron-sized three-dimensional porous support body and Y is enabled to be simultaneously used for carrying out Y-shaped porous support body through the mutual diffusion and restriction of multiple elements and the synergistic and sequential sectional sintering 2 O 3 The nano particles gradually react with the micron-sized three-dimensional porous support body, and a nanoscale three-dimensional reticular structure is constructed on the micron-sized three-dimensional porous support body, so that the micron/nanometer double-scale filtering membrane is formed. In addition, the invention can restrict the diffusion of various intermediate products formed after the diffusion of each element by controlling the heating rate and the heat preservation time of each sintering stage, thereby realizing the control of the aperture size of the filtering membrane, leading the aperture of the three-dimensional porous support body to be 1-100 microns and the aperture of the meter-level three-dimensional net to be 10-1000 nm.
Comparative example 1
The comparative example only differs from example 1 in that: the filtration treatment was not carried out using the filtration membrane of the present invention, and the other operations were the same as in example 1.
Comparative example 2
The comparative example is different from example 1 in that mechanical stirring was carried out without using the stirring apparatus of the present invention in the stirring treatment, and the other operations were the same as example 1.
Experimental part
In order to verify the removal effect of the impurities in the coal tar by the method, the method disclosed by the invention performs the following tests:
the invention adopts low-temperature coal tar produced by certain coking enterprises as a raw material, wherein the metals mainly comprise calcium, iron and sodium, and the contents of the metals are respectively 60.4 mug/g, 57.3 mug/g and 2.6 mug/g.
The method of examples 1 to 3 and comparative examples 1 and 2 are respectively used for treating the low temperature coal tar, and the treatment results are shown in Table 1.
TABLE 1 results of treatment
| Dehydration Rate (%) | Metal removal rate (%) | Dechlorination Rate (%) | Salt rejection (%) | |
| Example 1 | 96 | 95 | 65 | 88 |
| Example 2 | 94 | 92 | 63 | 85 |
| Example 3 | 91 | 88 | 60 | 82 |
| Comparative example 1 | 85 | 75 | 48 | 70 |
| Comparative example 2 | 88 | 86 | 57 | 79 |
In table 1, the demetallization rate was calculated based on the total mass of iron, calcium and sodium.
It is to be understood that the above-described embodiments are only some of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (7)
1. The method for removing impurities from coal tar is characterized by comprising the following steps:
filtering the coal tar through a filtering membrane, and uniformly stirring the filtered coal tar and the demetallization agent through a stirring device to convert a metal complex and organic chlorine in the coal tar into inorganic salt; then, adding water into the stirring device, and uniformly stirring to transfer the converted inorganic salt from the coal tar into a water phase to obtain a mixture; separating the mixture into three phases of solid, water and oil by a horizontal screw centrifuge, and then removing residual water by carrying out centrifugal flash evaporation treatment on the oil phase to obtain coal tar after impurities are removed;
the filter membrane is prepared by the following steps:
step 1, weighing the following preparation raw materials in parts by weight for later use: 45-50 parts of Al metal powder, 35-40 parts of Nb metal powder, 5-10 parts of Ti metal powder and Y 2 O 3 5-10 parts of nano particles;
step 2, al metal powder, nb metal powder, ti metal powder and Y 2 O 3 Carrying out dry ball milling on the nanoparticles for 4 to 20h in a ball mill with the ball-to-material ratio of 1 to 4 and the rotating speed of 50 to 250r/min to obtain mixed powder; pressing and molding the mixed powder under the pressure of 150 to 400MPa to obtain a pressed blank;
step 3, keeping the temperature of the pressed blank from room temperature to 120 ℃ at a heating rate of 3 to 5 ℃/min under a vacuum condition, keeping the temperature for 0.5 to 1.5 hours, then keeping the temperature for 3 to 5 hours at a heating rate of 2 to 4 ℃/min to 550 to 650 ℃, keeping the temperature for 3 to 5 hours, then keeping the temperature for 3 to 5 hours at a heating rate of 2 to 4 ℃/min to 850 to 950 ℃, keeping the temperature for 3 to 5 hours at a heating rate of 3 to 5 ℃/min to 1250 to 1350 ℃, keeping the temperature for 3 to 5 hours, and cooling to obtain the filtering membrane;
the demetallizing agent is polyamine carboxylate;
the dosage ratio of the demetallization agent to the coal tar is 100-200 mu g:1g.
2. The method for removing impurities from coal tar according to claim 1, wherein the stirring device comprises:
the device comprises a shell (1), wherein the upper end of the shell is provided with an oil inlet (11), an agent inlet (12), a water inlet mechanism (2) and a driving mechanism (3); a stirring mechanism (4) is arranged in the stirring device; and the lower end of the discharge hole is provided with a discharge hole (13);
the stirring mechanism (4) comprises a rotating rod (41), a plurality of stirring rods (42) and a plurality of wall scrapers (43);
the rotating rod (41) is vertically arranged in the shell (1), and the upper end of the rotating rod penetrates through the shell (1) to be in transmission connection with the driving mechanism (3);
the stirring rods (42) are arranged at equal intervals along the axial direction of the rotating rod (41), one end of each stirring rod (42) is fixedly connected with the rotating rod (41), and the other ends of every two adjacent stirring rods (42) in the vertical direction are fixedly connected with one side of one wall scraper (43); the other side of the wall scraper (43) is abutted against the side wall of the shell (1).
3. The method for removing impurities from coal tar according to claim 2, wherein the water inlet mechanism (2) comprises:
one end of the water inlet pipe (21) is used for connecting a water source, and the other end of the water inlet pipe is provided with a three-way valve (22);
the two flow guide pipes (23) are respectively arranged at two symmetrical water outlet ends of the three-way valve (22);
the two spray heads (24) are respectively arranged at the water outlet ends of the two flow guide pipes (23);
and the two first valve bodies (25) are respectively arranged on the two flow guide pipes (23) and are respectively positioned between the three-way valve (22) and the two spray heads (24).
4. The method for removing impurities from coal tar according to claim 2, wherein the stirring device further comprises a heating mechanism (5) and a heat dissipation mechanism (6);
the heating mechanism (5) comprises an electric heating sheet (51) and a temperature sensor (52), and the electric heating sheet (51) is sleeved on the inner wall of the shell (1); the temperature sensor (52) is arranged at the bottom of the inner side of the shell (1);
the heat dissipation mechanism (6) comprises a ventilation cavity (61), the ventilation cavity (61) is arranged between the electric heating sheet (51) and the outer wall of the shell (1), an air inlet (62) is formed in one end of the ventilation cavity (61), and an air outlet (63) is formed in the other end of the ventilation cavity (61); the air inlet (62) and the air outlet (63) are respectively provided with a second valve body (64) and a third valve body (65).
5. The method for removing impurities from coal tar according to claim 2, wherein an auxiliary stirring rod (44) is horizontally arranged at the lower end of the rotating rod (41).
6. The method for removing impurities from coal tar according to claim 1, wherein the metal remover is added, and then the mixture is stirred at a temperature of 75 to 85 ℃ for 0.5 to 3h at a speed of 250 to 350r/min.
7. The method for removing impurities from coal tar according to claim 1, wherein the coal tar is heated to 50-65 ℃ and then filtered by a filter membrane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111394481.5A CN113956899B (en) | 2021-11-23 | 2021-11-23 | Method for removing impurities from coal tar |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111394481.5A CN113956899B (en) | 2021-11-23 | 2021-11-23 | Method for removing impurities from coal tar |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113956899A CN113956899A (en) | 2022-01-21 |
| CN113956899B true CN113956899B (en) | 2022-12-02 |
Family
ID=79471660
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111394481.5A Active CN113956899B (en) | 2021-11-23 | 2021-11-23 | Method for removing impurities from coal tar |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113956899B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105214513A (en) * | 2015-11-04 | 2016-01-06 | 上海蓝科石化环保科技股份有限公司 | A kind of microfiltration membranes and utilize microfiltration membranes to purify the process of coal tar raw material |
| CN106929082A (en) * | 2017-04-06 | 2017-07-07 | 上海蓝科石化环保科技股份有限公司 | A kind of coal tar preprocess method and system |
| CN108044091A (en) * | 2017-12-07 | 2018-05-18 | 北京科技大学 | A kind of preparation of high-Nb Ti-Al base porous compound material filtration membrane and application process |
| CN111662746A (en) * | 2019-03-07 | 2020-09-15 | 中国科学院过程工程研究所 | Method for synchronously demetallizing, desalting and dehydrating coal tar |
| CN112940768A (en) * | 2021-04-01 | 2021-06-11 | 萍乡市新安环保工程有限公司 | Treatment method and treatment system for tar residues |
-
2021
- 2021-11-23 CN CN202111394481.5A patent/CN113956899B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105214513A (en) * | 2015-11-04 | 2016-01-06 | 上海蓝科石化环保科技股份有限公司 | A kind of microfiltration membranes and utilize microfiltration membranes to purify the process of coal tar raw material |
| CN106929082A (en) * | 2017-04-06 | 2017-07-07 | 上海蓝科石化环保科技股份有限公司 | A kind of coal tar preprocess method and system |
| CN108044091A (en) * | 2017-12-07 | 2018-05-18 | 北京科技大学 | A kind of preparation of high-Nb Ti-Al base porous compound material filtration membrane and application process |
| CN111662746A (en) * | 2019-03-07 | 2020-09-15 | 中国科学院过程工程研究所 | Method for synchronously demetallizing, desalting and dehydrating coal tar |
| CN112940768A (en) * | 2021-04-01 | 2021-06-11 | 萍乡市新安环保工程有限公司 | Treatment method and treatment system for tar residues |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113956899A (en) | 2022-01-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR100382122B1 (en) | Method for producing high purity terephthalic acid | |
| KR102629266B1 (en) | Methods, devices and systems for processing carbonaceous compositions | |
| CN201644093U (en) | Reaction and filter dryer | |
| CN207153705U (en) | A kind of reactor with solid-liquid separation function | |
| CN112979466B (en) | Application method of refining device of medicinal ethyl oleate | |
| CN206295869U (en) | A kind of industrial chemicals mixing stirring device for being easy to clean | |
| WO1996041855A1 (en) | Method of continuous extraction of crude wax and apparatus therefor | |
| DE102016101213A1 (en) | Apparatus and method for modifying porous solids | |
| CN113956899B (en) | Method for removing impurities from coal tar | |
| CN106732230A (en) | A kind of chemical mixing unit with knot screen | |
| CN102515295B (en) | Scraper demineralizer for supercritical water treatment of waste organic matters | |
| JPS61220723A (en) | Multifunctioned treating device | |
| CN117443085A (en) | Raw material separation equipment for processing new energy automobile cooling liquid | |
| CN1819985B (en) | Method for producing high purity terephthalic acid | |
| CN112960881A (en) | Method and system for breaking package of ultrasonic hot-washing oily sludge | |
| CN107875990A (en) | A kind of continuous alkaline cleaner and technique | |
| CN110743476B (en) | Multifunctional calcium hydroxide preparation tank and preparation method | |
| CN101318894B (en) | Separation purification method and apparatus for p-benzene dicarboxylic acid | |
| CN107814404A (en) | A kind of production method of cube nano-calcium carbonate | |
| JP6541240B2 (en) | Modular subunit for suspension crystallization system and suspension crystallization method using the modular subunit | |
| CN101428185A (en) | Horizontal roll-over type filtering, washing and drying machine | |
| CN112792045A (en) | Device and method for cleaning nano material | |
| CN201324555Y (en) | Novel horizontal tipping filtering, washing and drying machine | |
| CN111494978A (en) | Sublimation crystallization combined device for extracting natural caffeine | |
| CN212188918U (en) | Chemical production is with layering isolation equipment |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |